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Hydrochloric Acid → 4-[2,2-Bis(4-fluorophenyl)ethyl]pyridine hydrochloride

HRID 1460245
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1460245
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([C:17]2[CH:22]=[CH:21][C:20]([F:23])=[CH:19][CH:18]=2)(O)[CH2:9][C:10]2[CH:15]=[CH:14][N:13]=[CH:12][CH:11]=2)=[CH:4][CH:3]=1.[P].I.[ClH:26]>C(O)(=O)C.CO.CCOCC>[ClH:26].[F:23][C:20]1[CH:21]=[CH:22][C:17]([CH:8]([C:5]2[CH:4]=[CH:3][C:2]([F:1])=[CH:7][CH:6]=2)[CH2:9][C:10]2[CH:15]=[CH:14][N:13]=[CH:12][CH:11]=2)=[CH:18][CH:19]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 4

HCID 313Hydrochloric AcidHCID 24841Hydrogen iodideHCID 5462309PhosphorusHCID 15020359alpha,alpha-Bis(4-fluorophenyl)-4-pyridineethanol

Produkt 1

HCID 199830744-[2,2-Bis(4-fluorophenyl)ethyl]pyridine hydrochlorideAusbeute 87 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 176
Acetic Acid
Lösungsmittel
HCID 887MethanolLösungsmittel
HCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

A mixture of 15.05 g (0.048 mole) of α,α-bis(4-fluorophenyl)-4-pyridineethanol, 3.2 g (0.1 mole) of phosphorus and 50 ml of 56.9% hydrogen iodide in 150 ml of glacial acetic acid was heated at reflux for 11 hr. The solvent was removed in vacuo, and the residue was partitioned between methylene chloride and dilute sodium hydroxide. The methylene chloride solution was dried over magnesium sulfate, and the solvent was removed in vacuo to give an oil. This was dissolved in a mixture of methanol and ether, and an excess of ethereal hydrogen chloride was added. The solvent was removed in vacuo, and the residue was recrystallized from a mixture of acetonitrile and ether to give 13.89 g (87% yield) of title compound as a white, crystalline solid, mp 197°-199° C.

Aufarbeitung

  1. temperaturewas heated
  2. temperatureat reflux for 11 hr
  3. customThe solvent was removed in vacuo
  4. customthe residue was partitioned between methylene chloride and dilute sodium hydroxide
  5. dry with materialThe methylene chloride solution was dried over magnesium sulfate
  6. customthe solvent was removed in vacuo
  7. customto give an oil
  8. customThe solvent was removed in vacuo
  9. customthe residue was recrystallized from a mixture of acetonitrile and ether

Quellen und Nachweise

ORD-Eintrag
ord-ed7e1f09f45a4e02a3738e8c7dd0d436
Quelldatensatz
uspto-grants-1991_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05070087

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